N-Methylbenzylamine → 1-Chloroethyl benzyl(methyl)carbamate

HRID 57212ノート

反応式

HRID 57212 の反応式
[CH3:1][NH:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[C:11]([O:13][CH:14]([Cl:16])[CH3:15])=[O:12]>CCOC(C)=O.C([O-])(O)=O.[Na+]>[CH2:3]([N:2]([CH3:1])[C:11](=[O:12])[O:13][CH:14]([Cl:16])[CH3:15])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 7669N-MethylbenzylamineHCID 5213051-Chloroethyl chloroformate

生成物 1

HCID 668694551-Chloroethyl benzyl(methyl)carbamate収率 54.9%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a vigorously stirred suspension of N-methylbenzylamine (0.260 mL, 2 mmol) in EtOAc (3 mL) and 3 mL of saturated NaHCO3 solution was added 1-chloroethyl chloroformate (0.160 mL, 2 mmol). Effervescence was observed. Once gas production had ceased, the reaction mixture was diluted with hexanes (10 mL). The aqueous phase was removed and the organic phase was washed with brine (5 mL), dried and concentrated to give the crude product as an oil (˜0.250 g). The compound was used in the subsequent step without further purification.

後処理

  1. customThe aqueous phase was removed
  2. washthe organic phase was washed with brine (5 mL)
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-3f3b9b125a734d4983827319e999fc27
出典データセット
uspto-grants-2016_09
特許番号
US09434718B2

反応ノート

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